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#$Date: 2016-03-22 11:11:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178888 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/17/4111767.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4111767
loop_
_publ_author_name
'Rasmus D. Poulsen'
'Anders Bentien'
'Marie Chevalier'
'Bo B. Iversen'
_publ_contact_author_address
;University of Aarhus
Department of Chemistry
Laboratory of Inorganic Chemistry
Langelandsgade 140
DK-8000 Aarhus C
Denmark
;
_publ_contact_author_email       bo@chem.au.dk
_publ_contact_author_fax         '+458619 6199'
_publ_contact_author_name        'Professor Bo B. Iversen'
_publ_contact_author_phone       +4589423969
_publ_section_title
;
 Synthesis, Physical Properties, Multitemperature Crystal Structure, and
 20 K Synchrotron X-ray Charge Density of a Magnetic Metal Organic
 Framework Structure, Mn₃[C₈O₄H₄]₃(C₅H₁₁ON)₂
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9156
_journal_page_last               9166
_journal_paper_doi               10.1021/ja051233z
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C34 H34 Mn3 N2 O14'
_chemical_formula_sum            'C34 H34 Mn3 N2 O14'
_chemical_formula_weight         859.45
_chemical_name_common            MnDEF
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.3550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.0770(4)
_cell_length_b                   10.7280(2)
_cell_length_c                   17.3260(4)
_cell_measurement_reflns_used    7818
_cell_measurement_temperature    175
_cell_measurement_theta_max      38.36
_cell_measurement_theta_min      2.14
_cell_volume                     3535.67(13)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      175
_diffrn_measured_fraction_theta_full 0.798
_diffrn_measured_fraction_theta_max 0.798
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'ω and π'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8141
_diffrn_reflns_theta_full        38.88
_diffrn_reflns_theta_max         38.88
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SMART 1k'
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.899677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       trapezshaped
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.175
_exptl_crystal_size_rad          0.184
_refine_diff_density_max         1.220
_refine_diff_density_min         -1.789
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         8141
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0706P)²+20.2121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.2005
_reflns_number_gt                6002
_reflns_number_total             8141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja051233zsi20050224_053341.cif
_cod_data_source_block           final175k
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4111767
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.2500 0.53271(6) 0.5000 0.01588(11) Uani 1 2 d S . .
Mn2 Mn 0.42564(2) 0.43204(4) 0.53539(2) 0.01740(10) Uani 1 1 d . . .
O1 O 0.46145(11) 0.5568(2) 0.43740(12) 0.0226(4) Uani 1 1 d . . .
O2 O 0.34866(11) 0.5203(2) 0.43493(11) 0.0213(4) Uani 1 1 d . A .
O8 O 0.29763(12) 0.6608(2) 0.58110(12) 0.0260(4) Uani 1 1 d . A .
O9 O 0.40830(12) 0.5914(3) 0.60018(15) 0.0322(5) Uani 1 1 d . A .
O11 O 0.30020(12) 0.3813(2) 0.56623(12) 0.0259(4) Uani 1 1 d . A .
O12 O 0.39613(13) 0.3145(3) 0.63103(16) 0.0394(7) Uani 1 1 d . A .
C1 C 0.40033(13) 0.5680(3) 0.40437(13) 0.0165(4) Uani 1 1 d . . .
C2 C 0.38982(15) 0.6353(3) 0.32890(15) 0.0210(5) Uani 1 1 d . A .
C3 C 0.44293(16) 0.7101(3) 0.30374(18) 0.0268(6) Uani 1 1 d . . .
H3 H 0.4859 0.7153 0.3328 0.032 Uiso 1 1 calc R A .
C4 C 0.43214(17) 0.7228(3) 0.73524(19) 0.0290(6) Uani 1 1 d . . .
H4 H 0.4671 0.6701 0.7198 0.035 Uiso 1 1 calc R . .
C5 C 0.36945(15) 0.7343(3) 0.68993(16) 0.0220(5) Uani 1 1 d . A .
C6 C 0.31707(17) 0.8116(3) 0.71394(18) 0.0286(6) Uani 1 1 d . . .
H6 H 0.2752 0.8207 0.6833 0.034 Uiso 1 1 calc R . .
C7 C 0.32691(17) 0.6243(3) 0.28383(18) 0.0293(6) Uani 1 1 d . . .
H7 H 0.2912 0.5741 0.3003 0.035 Uiso 1 1 calc R A .
C8 C 0.35723(16) 0.6566(3) 0.61742(16) 0.0230(5) Uani 1 1 d . . .
C11 C 0.33080(15) 0.3303(3) 0.62491(17) 0.0243(5) Uani 1 1 d . . .
C12 C 0.28871(15) 0.2875(3) 0.68920(16) 0.0222(5) Uani 1 1 d . A .
C13 C 0.21720(16) 0.3109(3) 0.68646(18) 0.0289(6) Uani 1 1 d . . .
H13 H 0.1951 0.3514 0.6438 0.035 Uiso 1 1 calc R A .
C14 C 0.32165(16) 0.2260(4) 0.75261(19) 0.0308(7) Uani 1 1 d . . .
H14 H 0.3696 0.2095 0.7543 0.037 Uiso 1 1 calc R A .
O21 O 0.4308(2) 0.2709(3) 0.4621(2) 0.0325(7) Uani 0.899(4) 1 d P A 1
N21 N 0.3912(3) 0.0897(4) 0.4080(3) 0.0667(14) Uani 1 1 d . A 1
C21 C 0.3865(3) 0.1859(4) 0.4550(3) 0.0434(10) Uani 0.899(4) 1 d P A 1
H21 H 0.3478 0.1903 0.4844 0.052 Uiso 1 1 calc R A 1
C22 C 0.4488(4) 0.0820(5) 0.3560(4) 0.0686(17) Uani 1 1 d . A 1
H22A H 0.4631 0.1660 0.3438 0.082 Uiso 1 1 calc R A 1
H22B H 0.4308 0.0431 0.3080 0.082 Uiso 1 1 calc R A 1
C23 C 0.5115(5) 0.0123(8) 0.3865(5) 0.091(2) Uani 1 1 d . A 1
H23A H 0.5350 0.0580 0.4286 0.137 Uiso 1 1 calc R A 1
H23B H 0.5429 0.0015 0.3462 0.137 Uiso 1 1 calc R A 1
H23C H 0.4976 -0.0678 0.4047 0.137 Uiso 1 1 calc R A 1
C24 C 0.3319(5) -0.0021(7) 0.4006(4) 0.095(3) Uani 1 1 d . A 1
H24A H 0.2885 0.0408 0.4092 0.114 Uiso 1 1 calc R A 1
H24B H 0.3278 -0.0343 0.3481 0.114 Uiso 1 1 calc R A 1
C25 C 0.3403(5) -0.1048(7) 0.4534(5) 0.092(3) Uani 1 1 d . A 1
H25A H 0.3862 -0.1406 0.4506 0.139 Uiso 1 1 calc R A 1
H25B H 0.3051 -0.1667 0.4398 0.139 Uiso 1 1 calc R A 1
H25C H 0.3352 -0.0759 0.5051 0.139 Uiso 1 1 calc R A 1
C31 C 0.450(2) 0.210(4) 0.424(3) 0.0434(10) Uani 0.101(4) 1 d P A 3
O31 O 0.428(3) 0.253(4) 0.482(2) 0.0325(7) Uani 0.101(4) 1 d P A 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O8 Mn1 O8 99.18(13) . 2_556
O8 Mn1 O11 170.32(9) . 2_556
O8 Mn1 O11 89.15(9) 2_556 2_556
O8 Mn1 O11 89.15(9) . .
O8 Mn1 O11 170.32(9) 2_556 .
O11 Mn1 O11 83.01(13) 2_556 .
O8 Mn1 O2 92.22(8) . 2_556
O8 Mn1 O2 92.15(8) 2_556 2_556
O11 Mn1 O2 82.50(8) 2_556 2_556
O11 Mn1 O2 92.44(8) . 2_556
O8 Mn1 O2 92.15(8) . .
O8 Mn1 O2 92.22(8) 2_556 .
O11 Mn1 O2 92.44(8) 2_556 .
O11 Mn1 O2 82.50(8) . .
O2 Mn1 O2 173.26(12) 2_556 .
O9 Mn2 O31 168.5(10) . .
O9 Mn2 O21 173.02(14) . .
O31 Mn2 O21 10.9(9) . .
O9 Mn2 O1 91.90(9) . 5_666
O31 Mn2 O1 95.3(13) . 5_666
O21 Mn2 O1 94.78(13) . 5_666
O9 Mn2 O12 90.24(12) . .
O31 Mn2 O12 79.7(9) . .
O21 Mn2 O12 90.57(12) . .
O1 Mn2 O12 100.08(9) 5_666 .
O9 Mn2 O1 89.34(10) . .
O31 Mn2 O1 100.9(9) . .
O21 Mn2 O1 90.14(10) . .
O1 Mn2 O1 77.50(8) 5_666 .
O12 Mn2 O1 177.53(9) . .
O9 Mn2 O2 87.33(9) . .
O31 Mn2 O2 94.2(12) . .
O21 Mn2 O2 86.64(12) . .
O1 Mn2 O2 132.96(7) 5_666 .
O12 Mn2 O2 126.95(8) . .
O1 Mn2 O2 55.46(7) . .
C1 O1 Mn2 163.21(18) . 5_666
C1 O1 Mn2 94.23(15) . .
Mn2 O1 Mn2 102.50(8) 5_666 .
C1 O2 Mn1 152.6(2) . .
C1 O2 Mn2 90.56(16) . .
Mn1 O2 Mn2 98.54(7) . .
C8 O8 Mn1 129.4(2) . .
C8 O9 Mn2 138.0(2) . .
C11 O11 Mn1 155.7(2) . .
C11 O12 Mn2 99.74(19) . .
O1 C1 O2 119.6(2) . .
O1 C1 C2 120.0(2) . .
O2 C1 C2 120.4(2) . .
C7 C2 C3 119.6(3) . .
C7 C2 C1 120.3(2) . .
C3 C2 C1 120.1(3) . .
C2 C3 C4 120.2(3) . 8_564
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 8_564 .
C5 C4 C3 120.2(3) . 8_565
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 8_565 .
C4 C5 C6 119.6(3) . .
C4 C5 C8 119.6(3) . .
C6 C5 C8 120.7(3) . .
C5 C6 C7 120.2(3) . 8_565
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 8_565 .
C2 C7 C6 120.1(3) . 8_564
C2 C7 H7 119.9 . .
C6 C7 H7 119.9 8_564 .
O9 C8 O8 126.1(3) . .
O9 C8 C5 115.6(3) . .
O8 C8 C5 118.2(3) . .
O12 C11 O11 121.6(3) . .
O12 C11 C12 118.8(3) . .
O11 C11 C12 119.6(3) . .
C13 C12 C14 119.9(2) . .
C13 C12 C11 120.2(3) . .
C14 C12 C11 119.9(3) . .
C12 C13 C14 120.1(3) . 7_556
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 7_556 .
C12 C14 C13 120.0(3) . 7_556
C12 C14 H14 120.0 . .
C13 C14 H14 120.0 7_556 .
C21 O21 Mn2 125.9(3) . .
C21 N21 C22 120.5(4) . .
C21 N21 C24 118.8(6) . .
C22 N21 C24 120.2(5) . .
O21 C21 N21 123.9(5) . .
O21 C21 H21 118.1 . .
N21 C21 H21 118.1 . .
N21 C22 C23 115.6(6) . .
N21 C22 H22A 108.4 . .
C23 C22 H22A 108.4 . .
N21 C22 H22B 108.4 . .
C23 C22 H22B 108.4 . .
H22A C22 H22B 107.5 . .
C25 C24 N21 113.8(7) . .
C25 C24 H24A 108.8 . .
N21 C24 H24A 108.8 . .
C25 C24 H24B 108.8 . .
N21 C24 H24B 108.8 . .
H24A C24 H24B 107.7 . .
C31 O31 Mn2 136(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O8 2.120(2) .
Mn1 O8 2.120(2) 2_556
Mn1 O11 2.170(2) 2_556
Mn1 O11 2.170(2) .
Mn1 O2 2.2701(19) 2_556
Mn1 O2 2.2701(19) .
Mn2 O9 2.085(2) .
Mn2 O31 2.13(4) .
Mn2 O21 2.152(4) .
Mn2 O1 2.173(2) 5_666
Mn2 O12 2.189(2) .
Mn2 O1 2.306(2) .
Mn2 O2 2.386(2) .
O1 C1 1.265(3) .
O1 Mn2 2.173(2) 5_666
O2 C1 1.262(3) .
O8 C8 1.258(4) .
O9 C8 1.254(4) .
O11 C11 1.258(4) .
O12 C11 1.254(4) .
C1 C2 1.494(4) .
C2 C7 1.386(4) .
C2 C3 1.388(4) .
C3 C4 1.390(4) 8_564
C3 H3 0.9300 .
C4 C5 1.385(4) .
C4 C3 1.390(4) 8_565
C4 H4 0.9300 .
C5 C6 1.387(4) .
C5 C8 1.511(4) .
C6 C7 1.393(4) 8_565
C6 H6 0.9300 .
C7 C6 1.393(4) 8_564
C7 H7 0.9300 .
C11 C12 1.494(4) .
C12 C13 1.384(4) .
C12 C14 1.390(4) .
C13 C14 1.393(4) 7_556
C13 H13 0.9300 .
C14 C13 1.393(4) 7_556
C14 H14 0.9300 .
O21 C21 1.242(6) .
N21 C21 1.321(6) .
N21 C22 1.476(8) .
N21 C24 1.497(8) .
C21 H21 0.9300 .
C22 C23 1.474(10) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.433(11) .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C31 O31 1.22(6) .
